IS 14923:2001 (Reaffirmed - 2012) %7av77m n wllw~t s `[ 2, 2,41, 2, SI$w$$. \ m I (Ww) --fmTR (- -*?qq Indian Standard POLYMERIZED 1,2, DIHYDRO 2,2,4TRIMETHYL QUINOLINE (TMQ) -- SPECIFICATION ICS 83.040.20 @ BIS 2001 BUREAU OF IN DIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 July 2001 Price Group 4 Rubber Products Sectional Committee, PCD 13 FOREWORD This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Rubber Products Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council. Polymerized 1, 2 dihydro 2,2, 4-trimethyl quinoline (TMQ) is a general purpose, heat resistant antioxidant. It belongs to staining type of antioxidants and is recommended for black or dark coloured rubber goods only. TMQ is soluble in toluene, sparingly soluble in petroleum ether and insoluble in water. It disperses easily in rubber during compounding. TMQ is not recommended for use in foodstuffs applications. For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS 2:1960 `Rules for rounding off numerical values (revised).' The number of significant places tetained in the rounded off value should be the same as that of the specified value in this standard. IS 14923:2001 Indian Standard POLYMERIZED 1,2, DIHYDRO 2,2,4TRIMETHYL QUINOLINE (TMQ) -- SPECIFICATION 1 SCOI E SI Table 1 Requirements of TMQ characteristics Requirement (3) 80-% 0.3 0.4 This standard prescribes the requirements, methods of sampling and test for polymerized 1,2 dihydro 2,2,4trimethyl quinoline (TMQ) intended for use as an antioxidant in rubber compounds. 2 REFERENCES Tile following standards contains provisions which through reference in this text, constitutes provisions of this standard. At the time of publication, the edition indicated were valid. All standards are subject to revision, and parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated &low: 1SNo. 1675:1971 3399:1993 3660 (Part 8): 2000 Title Stearic acid, revision) technical @-st No. (2) (1) point,"C i) Softening (By ballandringmethod) by mass,Max ii) Ashpercent iii) Heatlosspercent by mass, Methadof Test, Ref to Annex (4) A B c 3.3 Compounding Performance Requirement The material when compounded and tested as given in Annex D shall have its properties comparable within the limits prescribed in D-1.l with those of the sample complying with the requirements of 3.1 and 3.2 and approved previously by the purchaser. 4 PACKING AND MARKING 4.1 Packing The material shall be securely closed packed in 20 or 25 kg packs of multiwalled paper bags or as agreed to between the purchaser and the supplier. 4.2 Marking 4.2.1 The packages shall be legibly marked with the following information: a) Manufacturers's name and registered trademark, if any; b) Name of the material; c) Net mass of the material; d) Lot and batch numben and e) Month and year of manufacture. 4.2.2 BE Certification Marking The packages may also be marked with the Standard Mark. 4.2.3 The use of the Standard Mark is governed by the provisions of the Bureau of Indian Stanahds Act, 1986 and the Rules and Regulations made thereunder. The details of conditions under which the licence for the use of the Standard Mark may be granted to manufacturers or producers maybe obtained from the Bureau of Indian Standards. Zinc oxide for rubber industry (first revision) Methods of test for natural rubbem Part 8 Mixing and vulcanizing of rubber in standard compound (NR:9) (second revision) Rubber, raw natural (third revision) Benzothiazyl-2-cyclohexyl sulphenamide (@ revision) 4588:1986 7069:1986 Methods of sampling and test for 7086 (Part 1): 1973 rubber compounding ingredients: Part 1 7497:1985 8851:1994 High abrasion furnace (HAF) carbon black @rst revision) Sul~hur for rubber industry -- Sp&ification @rst revision) - 3 REQUIREMENTS 3.1 Description The material shall be in golden yellow to dark brown heeds or pastilled. 3.2 The material shall comply with the requirements given in Table 1. 1 IS 14923:2001 5 SAMPLING CONFORMITY AND CRITERIA FOR 5.2 Number of Tests Tests for all the characteristics shall be conducted on a composite sample. 5.3 Criteria for Conformity The lot shall be declwed as conforming to the specification if all the test results of each of the individual samples satisfy the corresponding requirement and also meets the soecified requirements given in Annex D. 5.1 Sampling For the purpose of ascertaining the conformity of polymerized 1,2 dihydro 2,2,4 -trimethyl quinoline (TMQ) in a consignment to the specification, sampling as prescribed in IS 7086 (Part 1) shall be followed. . ANNEX A [Table 1, S1 No. (i)] SOFTENING POINT A-1 SIGNIFICANCE AND USE A-1.l In general, with materials of these types, softening does not take place at a definite temperature. As the temperature rises, these materials gradually and imperceptibly change from brittle or exceedingly thick and slow flowing materials to softer and less viscous liquids. For this reason, the determination of the softening point must be made by a fixed arbitrary and closely defined method if the results obtained are to be comparable. A-1.2 In this test method, the softening point is defined as the temperature at which a disk of the sample held within a horizontal ring is forced downward a distance of 2.54 cm under the weight of a steel ball as the sample is heated at,a prescribed rate in a water or glycerin bath. A-2 APPARATUS A-2.1 Ring - A brass-shouldered ring conforming to the dimensions shown in Fig, l(a). If desired, the ring may be attached by brazing or other convenient manner to a brass wire of about 13 B and S gauge 1.5 to 2.0 mm in a diameter as shown in Fig. 2 (a). A-2.2 Ball -- A steel ball, 9.53 mm in diameter, weighing between 3.45 and 3.55 g. A-2.3 Ball Centering Guide -- A guide for centering the ball, constructed of brass and having the general shape and dimensions illustrated in Fig. 1 (c), the use of which is optional. A-2.4 Container -- A glass vessel, capable of being heated not less than 85 mm in diameter and not less than 127 mm in depth from the bottom of the flare. A-2.5 Support For Ring and Thermometer -- Any convenient method for supporting the ring and thermometer may be used, provided it meets the following requirements. 2 A-2.5.1 Ring shall be supported in a substantially, horizontal position. A-2.5.2 When using the apparatus shown in Fig. l(d). The bottom of the ring shall be 25.4 mm above the horizontal plate below it; bottom surface of the horizontal plate shall be 12.7 to 19.05 mm above the bottom of the beaker and depth of liquid in the beaker shall be not less than 101.6 mm. A-2.5.3 When using the apparatus shown in Fig. 2(e); the bottom of the ring shall be 25.4 mm above the bottom of the beaker, with the bottom end of the rod resting on the bottom of the beaker, and depth of liquid in the beaker shall be not less than 102 mm [see Fig. 2 (a), (b) and (c).] A-2.5.4 In both assembles thermometer shall be suspended so that ~ bottom of the bulb is level with the bottom of the ring and within 12.7 mm but not touching the ring. For referee work no more than two rings shall be used. A-2.6 Thermometer, having range 30 to 200°C. A-2.7 Mechanical Stirrer--A two-bladed motor-driven stirrer attach to the bottom of a true vertical shaft may be used to ensure uniform heat distribution [see Fig. 2 (d) for dimensions]. The direction of shaft rotation shall move the liquid upward. The speed shall be within the range from 500 to 700 rpm. A-2.8 Hydraulic Press -- A hydraulic pqesscapable of maintaining sustained pressure up to 55 MPa, to be used alternative with the hammer. A-3 PREPARATION METHOD OF SAMPLE BY POUR Select a sample representtltive of the material under test. The sample shall consist of fresh broken lumps free of oxidized surfaces. For samples received as IS 14923:2001 A (a) SHOULDERD RING THIS DIAMETER TO BE TO PERMIT FULL 19mm INSERTION OF RING INSIDE DIAMETER FULL 23 TO SLIDE OVER RING 24 (c) --7 n BALL CENTERING 4J GUIDE ~ 5.5, v; 1 0 I 19 1111 0 5.5 I K :4 I (b) RIM; 67 7C I ~ J ~ `" HOLDER (d) ASSEMBLY All dimensions inmillimetn.s. RING, RINGHOLDER, BALL CENTERINGGUIDE AND ASSEMBLY OF FIG. 1 SHOULDERED APPARATUS SHOWING Two RINGS small lumps, scrape off the surface layer of the lumps immediately before using, avoiding inclusion of finely divided material or dust. Select a quantity at least twice that necessary to fill the desired number of rings, but in no case less than 40 g, and melt it immediately in a clean container, using an oven, hot plate, sand, or oil bath to prevent local overheating. Take care to avoid incorporating air bubbles in the sample, which must not be heated above the temperature necessary to pour the material readily without inclusion of air bubbles. The time fromthe beginning of heating to the pouring of the sample shall not exceed 15 min. Immediately before filling the rings, preheat them to `approximately the temperature at which the material ,9 to he poured. The rings, while being filled, should res~on an amalgamated brass plate. Pour the sample into the rings so as to leave an excess on cooling. After cooling a minimum of 30 rein, cut the excess material off cleanly with a slightly heated knife or spatula. In case the test is repeated, use a clean container and fresh sample. A-4 PROCEDURE A-4.1 Procedure for Material Having Softening 80"C or Below A-4.1.1 Assembly of Apparatus Fill the glass vessel, to a depth of not less than 101.6 mm and not more than 197.8 mm with freshly boiled distilled water at 5"C. Use water which has been cooled to not less than 45°C below the anticipated softening point but in no case lower than 5°C. Locate the axis of the stirrer shaft near the back wall of the beaker, with the blades clearing the wall and with the bottom of the blades 19.0 mm above the top of the ring. Unless the ball centering guide is to be used, make a slight indentation in the centre of the sample by pressing the ball or a rounded rod, slightly heated for h,d ma~rials, into the material at this point. Suspend the ring containing the sample in the water so that the lower surface of the filled ring is 25.4 mm above the upper surface of the lower horizontal plate [see Fig. 1 (d)], ivhich is at least 12.7 mm and not 3 IS 14923:2001 No. 13 BBS GAGE BRASS WIRE 6 25 d (a) BRASS RING AND WIRE II Ifa II i-l (b) PROPER POSITION OF BALL -. ... .. \ II II II Tti5 -% I I 1 I IJl (c) BOTTOM GUIDE FOR WIRE I (e) c 0 e ASSEMBLY OF APPARATUS All dimensions in millimetres. FIG. 2 ASSEMBLY OF APPARATUS SHOWING STIRRERAND SINGLE SHOULDERED RING more than 19.0 mm above the bottom of the glass vessel or 25.4 above the bottom of the glass container [see Fig. 2 (e)]. Place the ball in the water but not on the test specimen. Suspend a low-softening point thermometer so that the bottom of its bulb is level with the bottom of the ring and within 12.7 mm but not touching the ring. Maintain the initial temperature of the water for 15 min. With suitable forceps, place the ball in the centre of the upper surface of the material in the ring. Start stirring and continue the stirring at 500 to 700 rpm until completion of determination. A-4.L2 Heating Apply heat in such a manner that the temperature of the water is raised 5°C/min. Avoid the effect of drafti 4 using shields if necessary. A-4.1.3 Permissibh Variation in Rise of Temperature The rate of rise of temperature shall be uniform and shall not be averaged over the period of the test. The maximum permissible variation for any minute period after the first three shall be f 0.5 `C. Reject all tests in which the rate of rise exceeds these limits. A-4.1.4 Sojlening Point Record as the softening point the temperature of the thermometer at the instant the material touches the lower horizontal plate [see Fig. 1 (d)], or the bottom of the container [see Fig. 2 (e)]. Make no correction for the emergent stem of the thermometer. IS 14923:2001 A-4.2 Procedure for Materials Having Softening Points above 80°C Use the same procedure as described in 5.1, except fill the bath with glycerin (Note 3) and use a high softening point thermometer. The starting temperature of the glycerin bath shall be 32"C, but for resins (including rosin) use glycerin that has been cooled to not less than 27°C below the anticipated softening point, but in no case lower than 35"C. NOTE -- For materials softening around SO"Creport the nature of the bath, and whether water or glycerin was used since a glycerine bath yields slightly higher results than a water bath. prescribed rate of beating is absolutely essential for reproducibility of results. A-5.3 In Fig. 1 (b), a thin amalgamated copper plate placed on the bottom lower plate of the ring holder will prevent the material from sticking there by saving considerable time and trouble in cleaning. A-5.4 Owing to possible danger to health if mercury is handled carelessly, the following rules should be observed at all times. A-5.4.1 Store, the mercury in a closed jug in a cool place. A-5.4.2 Strictly avoid spilling any mercury. A-5.4.3 Remove mercury vapours by working under a suitable hood with good ventilation. A-5.4.4 Keep amalgamated brass plates and other apparatus at no higher than normal room temperature. A-5 PRECAUTIONS A-5.1 The stirrer motor shall be so mounted that any vibrations created by its rotation are not conveyed directly to the sample support. A-5.2 The use of freshly boiled distilled water is essential as otherwise air bubbles may form on the specimen and affect the result. Rigid adherence to the ANNEX B [Table 1, S1 No. (ii)] DETERMINATION B-1 SCOPE This test method describes the determination of ash content of rubber chemicals. B-2 TERMINOLOGY B-2.1 Lot Sample A production sample representative of a standard production units, normally referred to as `the sample'. B-2.2 Test Unit The actual material used in the analysis. It must be representative of the `lot' sample, B-3 SUMMARY OF TEST METHODS B-3.1 The ash content is determined by heating a known quantity of the robber chemical on a hot plate or over a gas burner to volatilize the sample and then heating in a muffle furnace to complete the ashing process. B-3.2 The ash content is determined by heating a known quantity of the rubber chemical on a hot plate or over a gas burner to volatilize the sample and then heating in a muffle furnace to complete the ashing process. B-4 SIGNIFICANCE AND USE This test method is suitable for the determination of the ash content of robber chemicals. The test methods 5 OF ASH may be used for quality control, product acceptance, or research and development. B-5 APPARATUS B-5.1 Muffle Furnace, capable of temperature regulation of* 25°C between 500 and 800°C. B-5.2 Hot Plate (or Laboratory B-5.3 Laboratory Fume Hood B-5.4 Porcelain Combustion form 25 ml capacity. Crucible, capsule Gas Burner) B-5.5 Porcelain Crucible, high form size O, 15 ml capacity B-5.6 Clay Triangle B-5.7 Steel Crucible Tongs B-5.8 Heat Resistant Gloves B-5.9 Dessicator B-5.1O Analytical Balance, sensitive to 0.0001 g. B-5.11 Air Circulating Oven, capable of 70 * 2"C. B-6 PROCEDURE Ignite the 15 ml capacity crucible in the muffle furnace at 750* 25°C for 2 hours. Transfer the crucible to the desiccator, cool to room temperature and weigh to the nearest 0.000 1 g. Weigh a 5 g test sample to the IS 14923:2001 nearest 0.000 1 gintothe ignite procedure and place the crucible in the clay try angle carefully heat the crucible and content with the gas burner until all volatile material and pyrolysis products have been removed (gases may flame) and the residue has been carbonized. Transfer the crucible to the muffle furnace at 750 ~ 25°C and ignite for 2 h. Carefully transfer the crucible containing the ash to the desiccator, cool toroomtemperature and reweigh to the nearest 0.0001 g. Calculate the percent ash to the nearest 0.01 percent as follows: ~ = (l?q -rrq) (m*--m,) where " A ml mz = ash, percent; = massofcrucible, g; = mass ofcmcible plustest sample, gand; x 100 B-7 CALCULATION m~ = mass ofcrucible plus ash, g. ANNEX C [Tatie DETERMINATION C-1 SCOPE This test method covers the measurement of the loss of volatiles from sulphur at 70°C. Volatile components consist of moisture, low boiling organic components and TMQ. C-2 SUMMARY OF TEST METHOD The sulphur specimen is weighed before and after heating for 2 h at 70°C. The measured loss of mass is the volatile material content. C-3 SIGNIFICANCE AND USE This test method determines the volatile material in TMQ at 70°C. By ascertaining that the volatiles are lower than a predicted maximum limit, it may safely be concluded that moisture is below that limit and is not present in excessive amounts. Testing at temperature higher than 70°C only results in greater volatilization of TMQ. C-4 APPARATUS C-4.1 Weighing Bottle, low `form 82 ml capacity. C-4.2 Oven, explosion-proof, vented air circulating oven, capable of temperature regulation of 70 t 2"C. C-4.3 Analytical Balance, sensitive to 0.1 mg. C-7 REPORT Report results obtained from two individual determinations and their average to the nearest 0.01 percent. 1, S1 No. (iii)] OF VOLATILE MATERIAL C-4.4 Desiccator C-5 PROCEDURE Weigh the weighing bottle to the nearest 0.1 mg. Then add approximately 5 g TMQ and weigh again. Make sure that TMQ evenly covers the base of the bottle. Place the uncovered bottle in the 70"C oven for 2 h. Remove the specimen, cover and cool in a desiccator for 1 h. Weigh the cooled specimen to the nearest 0.1 mg. C-6 CALCULATION The volatile material is given the following equation: Jnl-m2}x1m ml where v= ml mz volatiles percent, = original specimen mass, and = heated specimen mass. 6 IS 14923:2001 ANNEX (Clauses D 3.3 and 5.3) METHOD FOR COMPOUNDING AND TESTING POLYMERIZED 1,2 DIHYDRO 2~,4-TRIMETHYL QUINOLINE (TMQ) D-1 TEST COMPOUND D-1.1 For guidance, the test compound with the following composition may be used for testing performance properties of TMQ in rubber compound Item Natural rubber grade IS NR 5, see IS 4588 Zinc oxide, see IS 3399 Stearic acid, see IS 1675 HAF carbon black, see IS 7497 Sulphur, see IS 8851 Parts by mass 100.0 5.0 2.0 35.0 2.25 D-3 TESTS D-3.1 The tests given below are recommended for each test sample. The approved sample shall also be tested in the same compound side by side. D-3.1.1 Tensile strength, modulus of 300 percent elongation and elongation at break at different cures at 141°C stepwise, from below to above the expected optimum cure, shall be determined to ascertain the optimum cure time. Tensile properties (that is tensile strength and elongation at break) of the vulcanizates cured at the ascertained optimum cure time are determined both before and after heat ageing at 70°C for 2,4 and 6 days. D-4 RESULTS The tensile strength and elongation at break, both of original sample and the aged samples shall be within +10 percent of the values obtained with the approved sample tested at the same time. J3enzothiazyl-2+yclohexylsulphenamide, 0.6 see IS 7069 TMQ D-2 COMPOUND FO11OW the procedure prescribed in NR: of IS 3660 (Part 8). 1.0 Bureau of Indian Standards BIS is a statutory institution established under the Bureau oj Indian Standards Act, 1986 to promote harmonious development of the activities of stardardization, marking and quality certification of goods and attend ing to connected matters in the country. Copyright BIS has the copyright of all its publications. No part of these publications may be reproduced in any form without the prior permission in writing of BIS. This does not preclude the free use, in the course of implementing the standard, of necessary details, such as symbols and sizes, type or grade designations. Enquiries relating to copyright be addressed to the Director (Publication), BIS Review of Indian Standards Amendments are issued to standards as the need arises on the basis of comments. 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